반응 #4999

반응 방정식

potassium carbonate

methyl 2-[(4,6-dimethoxypyrimidin-2-yl)thio]-6-acetylbenzoate

methoxyamine hydrochloride

water

→

aimed compound

수율 60.0%

methyl 2-[(4,6-dimethoxypyrimidin-2-yl)thio]-6-[1-(N-methoxyimino)ethyl]benzoate

수율 60.0%

용매

methanol

반응 조건

후처리

1. 1
   온도the resultant liquor was heat-refluxed for 3 hours
2. 2
   기타an oily product thus precipitated
3. 3
   추출was extracted with ethyl acetate
4. 4
   세척The ethyl acetate layer was washed with water
5. 5
   기타was dried
6. 6
   workup.DISTILLATIONto distill off ethyl acetate under reduced pressure
7. 7
   기타The residue thus obtained
8. 8
   기타was purified by chromatography

실험 절차

1.0 g of methyl 2-[(4,6-dimethoxypyrimidin-2-yl)thio]-6-acetylbenzoate and 0.5 g of methoxyamine hydrochloride were dissolved in 6 ml of methanol, and the resultant solution was refluxed for 15 minutes. After cooling the mixed liquor to room temperature, 0.8 g of potassium carbonate was added to this liquor and the resultant liquor was heat-refluxed for 3 hours. The reaction liquor was poured into a large amount of water, and an oily product thus precipitated was extracted with ethyl acetate. The ethyl acetate layer was washed with water, and was dried to distill off ethyl acetate under reduced pressure. The residue thus obtained was purified by chromatography to obtain 0.65 g of the aimed compound (refractive index=1.5709) at a yield of 59%.

출처